CN114054054B - Ternary visible light photocatalysis nano composite material and preparation method thereof - Google Patents

Ternary visible light photocatalysis nano composite material and preparation method thereof Download PDF

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CN114054054B
CN114054054B CN202111495191.XA CN202111495191A CN114054054B CN 114054054 B CN114054054 B CN 114054054B CN 202111495191 A CN202111495191 A CN 202111495191A CN 114054054 B CN114054054 B CN 114054054B
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CN114054054A (en
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李明
山传福
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Guilin University of Technology
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    • B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
    • B01J27/14—Phosphorus; Compounds thereof
    • B01J27/16—Phosphorus; Compounds thereof containing oxygen, i.e. acids, anhydrides and their derivates with N, S, B or halogens without carriers or on carriers based on C, Si, Al or Zr; also salts of Si, Al and Zr
    • B01J27/18—Phosphorus; Compounds thereof containing oxygen, i.e. acids, anhydrides and their derivates with N, S, B or halogens without carriers or on carriers based on C, Si, Al or Zr; also salts of Si, Al and Zr with metals other than Al or Zr
    • B01J27/1802—Salts or mixtures of anhydrides with compounds of other metals than V, Nb, Ta, Cr, Mo, W, Mn, Tc, Re, e.g. phosphates, thiophosphates
    • B01J27/1817—Salts or mixtures of anhydrides with compounds of other metals than V, Nb, Ta, Cr, Mo, W, Mn, Tc, Re, e.g. phosphates, thiophosphates with copper, silver or gold
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/72—Treatment of water, waste water, or sewage by oxidation
    • C02F1/725—Treatment of water, waste water, or sewage by oxidation by catalytic oxidation
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
    • B01J21/06—Silicon, titanium, zirconium or hafnium; Oxides or hydroxides thereof
    • B01J21/063—Titanium; Oxides or hydroxides thereof
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
    • B01J21/18—Carbon
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    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
    • B01J23/38—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals
    • B01J23/48—Silver or gold
    • B01J23/50—Silver
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J35/00—Catalysts, in general, characterised by their form or physical properties
    • B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
    • B01J35/39—Photocatalytic properties
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    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
    • B01J37/02—Impregnation, coating or precipitation
    • B01J37/0201—Impregnation
    • B01J37/0207—Pretreatment of the support
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    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
    • B01J37/02—Impregnation, coating or precipitation
    • B01J37/0215—Coating
    • B01J37/0217—Pretreatment of the substrate before coating
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    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/30—Treatment of water, waste water, or sewage by irradiation
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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    • C02F2305/08—Nanoparticles or nanotubes
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    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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    • C02F2305/00—Use of specific compounds during water treatment
    • C02F2305/10—Photocatalysts

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Abstract

The invention discloses a ternary visible light photocatalysis nano composite material and a preparation method thereof, belonging to the technical field of functional materials, and comprising the following steps: s1, preparing phosphorus-doped graphene quantum dots, wherein pyrene and nitric acid are used as raw materials to prepare trinitropyrene; adding water into the trinitropyrene, adding a phosphorus source, adjusting the pH to 10-11, and carrying out hydrothermal reaction at 180 ℃ to prepare a phosphorus doped graphene quantum dot; s2, preparing an S1 phosphorus doped graphene quantum dot aqueous solution, mixing with titanium dioxide nano particles, silver nitrate and potassium iodide, filtering, and drying to prepare a ternary visible light photocatalytic nanocomposite; the prepared nano material is put into methyl orange solution, and under the irradiation of visible light, the catalytic efficiency can reach 99.35% within 10 minutes, and the nano material shows excellent catalytic performance.

Description

Ternary visible light photocatalysis nano composite material and preparation method thereof
Technical Field
The invention belongs to the technical field of functional materials, and particularly relates to a ternary visible light photocatalysis nanocomposite and a preparation method thereof.
Background
The pollution of organic dye water brings great hidden trouble to the health and life of people, and has become a serious challenge worldwide. Semiconductor photocatalysis is a very promising approach to solve this problem. In semiconductor multi-component photocatalysis, various refractory pollutants from the environment are decomposed under ultraviolet/visible light irradiation, titanium dioxide is the most potential one of the known photocatalysis semiconductor materials studied, and has the characteristics of stable performance, no toxicity, low cost and the like, and is widely applied to various fields since 1972 when being applied to water decomposition for the first time. However, drawbacks such as a wide band gap, high recombination rate of carriers, etc. limit their photocatalytic efficiency. The existing preparation method of the photocatalysis composite material with titanium dioxide as a main component only has the catalytic degradation effect on organic dye dirt in water under ultraviolet light, but has poor catalytic effect in a visible light wavelength region, has extremely low utilization rate on solar energy, and is difficult to realize large-scale commercial use.
Disclosure of Invention
In order to solve the technical problems, the invention provides a ternary visible light photocatalysis nano composite material and a preparation method thereof, titanium dioxide nano-scale particles, phosphorus doped graphene quantum dots and silver iodide are combined into the nano composite material by a simple method, the phosphorus doped graphene quantum dots are introduced into the surface of the titanium dioxide to improve the photosensitization of the titanium dioxide, and form P/N sections with the titanium dioxide to obviously improve the carrier transmission reduction and the photo-generated electron recombination, the silver iodide and the titanium dioxide are coupled to construct a heterojunction to form interface energy deviation between the semiconductor surfaces, the charge hole separation efficiency can be increased, and the silver iodide has strong absorption capacity on the visible light radiation absorption; the composite material can efficiently utilize sunlight to decompose different organic pollutants in water.
The invention is realized by the following technical scheme.
The first object of the invention is to provide a preparation method of ternary visible light photocatalysis nano composite material, comprising the following steps:
s1, preparation of phosphorus doped graphene quantum dots
Using pyrene and nitric acid as raw materials to prepare trinitropyrene; adding water into the trinitropyrene, adding a phosphorus source, adjusting the pH to 10-11, and carrying out hydrothermal reaction at 180 ℃ to prepare a phosphorus doped graphene quantum dot;
s2, preparing an S1 phosphorus doped graphene quantum dot aqueous solution, mixing with titanium dioxide nano particles, silver nitrate and potassium iodide, filtering, and drying to prepare the ternary visible light photocatalysis nano composite material.
Preferably, in S1, the ratio of pyrene to nitric acid is 1g:100mL.
Preferably, in S1, the trinitropyrene is prepared by heating, refluxing and stirring for 12 hours in a water bath at 80 ℃.
Preferably, in S1, the phosphorus source is disodium hydrogen phosphate dodecahydrate.
Preferably, in S1, trinitropyrene: water: the phosphorus source was obtained in an amount ratio of 1mg:1mL:0.03g.
Preferably, in S1, the time of the hydrothermal reaction is 6 hours.
Preferably, in S1, after the hydrothermal reaction is completed, the solution is dialyzed for 24 to 36 hours using a dialysis bag having a molecular weight cut-off of 3500Da, and then dried.
Preferably, in S2, the raw materials are smoothly added as follows: dispersing titanium dioxide nano particles in a phosphorus doped graphene quantum dot aqueous solution, adding silver nitrate, uniformly mixing, and dropwise adding a potassium iodide aqueous solution in the stirring process.
Preferably, in S2, the concentration of the phosphorus doped graphene quantum dot aqueous solution is 0.2mg/mL, and the titanium dioxide nano particles: phosphorus doped graphene quantum dot aqueous solution: silver nitrate: the dosage ratio of potassium iodide is 0.5g:500mL:0.097g:0.092g.
A second object of the present invention is to provide a ternary visible light photocatalytic nanocomposite prepared by the above preparation method.
Compared with the prior art, the invention has the following beneficial effects:
(1) According to the invention, the titanium dioxide nano-scale particles, the phosphorus doped graphene quantum dots and the silver iodide are combined into the nano composite material, and the titanium dioxide, the phosphorus doped graphene quantum dots and the silver iodide are successfully compounded into the ternary nano material by simply dissolving in water and stirring a suspension for adsorption during the synthesis of the nano composite material, so that the method does not use modes such as heating, and the cost is low and the operation is convenient.
(2) The prepared nano material is put into methyl orange solution, and under the irradiation of visible light, the catalytic efficiency can reach 99.35% within 10 minutes, and the nano material shows excellent catalytic performance.
Drawings
FIG. 1 is a TEM image of the P25/PCDs/AgI material prepared in example 1;
FIG. 2 is a HRTEM diagram of the P25/PCDs/AgI material prepared in example 1;
FIG. 3 is a FESEM image of the P25/PCDs/AgI material prepared in example 1;
FIG. 4 is an EDS diagram of the P25/PCDs/AgI material prepared in example 1;
FIG. 5 is an XPS spectrum of the P25/PCDs/AgI material prepared in example 1;
FIG. 6 is a graph showing the catalytic performance of the materials of example 1 and comparative examples 1 to 4 on methyl orange.
Detailed Description
In order that those skilled in the art will better understand the technical solution of the present invention, the present invention will be further described with reference to the specific examples and the accompanying drawings, but the examples are not intended to be limiting.
The experimental methods and the detection methods described in the following examples are all conventional methods unless otherwise specified; the reagents and materials are commercially available unless otherwise specified.
Example 1
A preparation method of a ternary visible light photocatalysis nano composite material comprises the following steps:
(1) After 1g of pyrene and 100ml of nitric acid are mixed, the mixture is heated in a water bath at 80 ℃ to reflux and stir for 12 hours, reactants are added into 500ml of purified water to be filtered, yellow solid which is trinitropyrene is obtained, 40mg of trinitropyrene is put into 40ml of water, 1.2g of disodium hydrogen phosphate dodecahydrate is added as a phosphorus source, sodium hydroxide is added to enable the pH value of the mixed solution to reach 10, the mixed solution is placed into a 100ml reaction kettle, and the mixed solution is heated for 6 hours at 180 ℃. After cooling, the solution was filtered and dialyzed for 24 hours using 3500Da dialysis bags, and the dialyzed solution was cooled and dried to obtain phosphorus doped graphene quantum dots (PCDs).
(2) Taking 0.5g of commercial grade titanium dioxide nano particles (P25), dispersing in 500ml of (0.2 mg/ml) phosphorus doped graphene quantum dot aqueous solution, rapidly magnetically stirring for 0.5h, putting 0.097g of silver nitrate into the mixed solution, rapidly magnetically stirring for one hour, then dissolving 0.092 potassium iodide into 20ml of water, dropwise adding into the mixed solution, dropwise adding the mixed solution while stirring to find that the color is obviously changed into yellow green, filtering at 60 ℃ and drying to obtain the novel ternary excellent visible light photocatalytic nanocomposite (P25/PCDs/AgI) (titanium dioxide, phosphorus doped graphene quantum dots and silver iodide).
Example 2
(1) After 1g of pyrene and 100ml of nitric acid are mixed, the mixture is heated in a water bath at 80 ℃ to reflux and stir for 12 hours, reactants are added into 500ml of purified water to be filtered, yellow solid which is trinitropyrene is obtained, 40mg of trinitropyrene is put into 40ml of water, 1.2g of disodium hydrogen phosphate dodecahydrate is added as a phosphorus source, sodium hydroxide is added to enable the pH value of the mixed solution to reach 11, the mixed solution is placed into a 100ml reaction kettle, and the mixed solution is heated for 6 hours at 180 ℃. And (3) cooling, filtering to obtain a solution, dialyzing the solution for 36 hours by using a 3500Da dialysis bag, and cooling and drying the dialyzed solution to obtain the phosphorus doped graphene quantum dot.
(2) Taking 0.5g of commercial grade titanium dioxide nano particles (P25), dispersing in 500ml of (0.2 mg/ml) phosphorus doped graphene quantum dot aqueous solution, rapidly magnetically stirring for 0.5h, putting 0.097g of silver nitrate into the mixed solution, rapidly magnetically stirring for one hour, then dissolving 0.092 potassium iodide into 20ml of water, dropwise adding into the mixed solution, dropwise adding the mixed solution while stirring to find that the color is obviously changed into yellow green, filtering at 60 ℃, and drying at the temperature to obtain the novel ternary excellent visible light photocatalytic nano composite material (titanium dioxide, phosphorus doped graphene quantum dots and silver iodide).
Comparative example 1
Dispersing titanium dioxide nano particles (P25) in 500ml (0.2 mg/ml) of the phosphorus doped graphene quantum dot aqueous solution prepared in the step (1) of the example 1, rapidly magnetically stirring for 0.5h, filtering, and drying at 60 ℃ to prepare the P25/PCDs material.
Comparative example 2
And (3) rapidly magnetically stirring the P25 and the pure graphene quantum dot aqueous solution dispersed in 500ml of 0.2mg/ml for 0.5h, filtering, and drying at 60 ℃ to obtain the P25/CDs material.
Comparative example 3
Dispersing P25 in 500ml of 0.2mg/ml pure graphene quantum dot aqueous solution, rapidly magnetically stirring for 0.5h, putting 0.097g of silver nitrate into the mixed solution, rapidly magnetically stirring for one hour, dissolving 0.092 potassium iodide into 20ml of water, dropwise adding into the mixed solution, filtering, and drying at 60 ℃ to obtain the P25/CDs/AgI material.
Comparative example 4
Titanium dioxide nanoparticles (P25).
The materials prepared in examples 1 and 2 have similar properties, and the materials prepared in example 1 are characterized first, in which fig. 1 is a TEM image of P25/PCDs/AgI material, fig. 2 is an HRTEM image of P25/PCDs/AgI material, and from fig. 2, three lattice spacings, a planar lattice spacing of 0.35nm corresponds to P25, a planar lattice spacing of 0.231nm corresponds to AgI, and a planar lattice spacing of 0.243 corresponds to PCDs, thus proving successful synthesis of the composite material; fig. 3 is a FESEM view of the material, as can be taken from fig. 1 and 3, with TEM and FESEM images of the material fitting each other to a high degree, which shows that the nanocomposite is almost composed of spherical particles, and particle agglomeration is observed due to the high growth of the nanocomposite. FIG. 4 is an EDS chart of a material, FIG. 5 is an XPS spectrum chart of a material, and it is clear from FIGS. 4 and 5 that the three-way catalyst sample contains C, P, ag, I, TI, O elements, illustrative PCDs, agI, TIO 2 A three-way photocatalyst with stable structure is constructed by physical adsorption.
The performance of the P25/PCDs/AgI prepared in example 1 was characterized by the following procedure with reference to comparative examples 1 to 4:
0.1g of the catalysts of example 1 and comparative examples 1 to 4, respectively, was put into a 10mg/L methyl orange solution and sonicated in the dark for one hour to reach adsorption equilibrium. Under 300w visible light, 5ml of the sample solution was filtered every five minutes to test the methyl orange concentration in the solution. Specific results are shown in FIG. 6, and the results of FIG. 6 show that the material prepared in example 1 has a catalytic efficiency of 99.35% in 10 minutes under irradiation of visible light, and shows excellent catalytic performance, compared with those of comparative examples 1 to 4.
It will be apparent to those skilled in the art that various modifications and variations can be made to the present invention without departing from the spirit or scope of the invention. Thus, it is intended that such modifications and variations be included herein within the scope of the appended claims and their equivalents.

Claims (9)

1. The preparation method of the ternary visible light photocatalysis nano composite material is characterized by comprising the following steps of:
s1, preparation of phosphorus doped graphene quantum dots
Using pyrene and nitric acid as raw materials to prepare trinitropyrene; adding the trinitropyrene into water, adding a phosphorus source, adjusting the pH to 10-11, and carrying out hydrothermal reaction at 180 ℃ to prepare a phosphorus doped graphene quantum dot;
s2, dispersing titanium dioxide nano particles in a phosphorus doped graphene quantum dot aqueous solution, adding silver nitrate, uniformly mixing, dropwise adding a potassium iodide aqueous solution in the stirring process, filtering, and drying to prepare the ternary visible light photocatalytic nanocomposite compounded by titanium dioxide, phosphorus doped graphene quantum dots and silver iodide.
2. The method for preparing the ternary visible light photocatalytic nanocomposite according to claim 1, wherein in S1, the ratio of pyrene to nitric acid is 1g:100mL.
3. The method for preparing the ternary visible light photocatalytic nanocomposite according to claim 1, wherein in S1, the preparation of the trinitropyrene is performed by heating and refluxing in a water bath at 80 ℃ for 12 hours.
4. The method for preparing a ternary visible light photocatalytic nanocomposite according to claim 1, wherein in S1, the phosphorus source is disodium hydrogen phosphate dodecahydrate.
5. The method for preparing a ternary visible light photocatalytic nanocomposite material according to claim 1, wherein in S1, trinitropyrene: water: the phosphorus source dosage ratio was 1mg:1mL:0.03g.
6. The method for preparing a ternary visible light photocatalytic nanocomposite material according to claim 1, wherein in S1, the time of the hydrothermal reaction is 6 hours.
7. The method for preparing a ternary visible light photocatalytic nanocomposite according to claim 1, wherein in S1, after the completion of the hydrothermal reaction, the solution is dialyzed for 24 to 36 hours using a dialysis bag having a molecular weight cut-off of 3500Da, and then dried.
8. The preparation method of the ternary visible light photocatalytic nanocomposite according to claim 1, wherein in S2, the concentration of the phosphorus doped graphene quantum dot aqueous solution is 0.2mg/mL, and the titanium dioxide nanoparticles: phosphorus doped graphene quantum dot aqueous solution: silver nitrate: the dosage ratio of potassium iodide is 0.5g:500mL:0.097g:0.092g.
9. A ternary visible light photocatalytic nanocomposite prepared according to the preparation method of any one of claims 1 to 8.
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